Potassium Carbonate → 1-Benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine

HRID 352778노트

반응식

HRID 352778 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([S:14](=[O:17])(=[O:16])[NH2:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:19][C:20]1[CH:21]=[C:22]([Cl:28])[CH:23]=[CH:24][C:25]=1[CH2:26]Br.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][N:11]([S:14]([N:15]2[CH:19]=[C:20]3[C:25]([CH:24]=[CH:23][C:22]([Cl:28])=[CH:21]3)=[CH:26]2)(=[O:17])=[O:16])[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 112305864-Benzylpiperazine-1-sulfonamideHCID 150082261,2-Bis(bromomethyl)-4-chlorobenzene

생성물 1

HCID 227101621-Benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In ethanol (5 ml), 1-benzyl-4-sulfamoylpiperazine (251 mg) was dissolved. To the resulting solution, 3,4-bis(bromomethyl)-1-chlorobenzene (293 mg) and potassium carbonate (204 mg) were added, followed by heating under reflux for 3.5 hours. After cooling, the precipitate was filtered off. The filtrate was then distilled under reduced pressure and the residue was purified by chromatography on a silica gel column (dichloromethane˜ethanol:dichloromethane=1:100), whereby the title compound (222 mg, 58%) was obtained.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 3.5 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitate was filtered off
  5. distillationThe filtrate was then distilled under reduced pressure
  6. customthe residue was purified by chromatography on a silica gel column (dichloromethane˜ethanol:dichloromethane=1:100), whereby the title compound (222 mg, 58%)
  7. customwas obtained

출처 및 근거

ORD 기록
ord-27d20b4baceb48d0b7bfa6089b63ecb4
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747023B1

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